Luminescent Thermometry by a Y/Eu Binary Layered Rare-Earth Hydroxide (LRH) via In Situ Intercalation with Neutral Terbium(III) Complexes

Article abstract of DOI:10.1002/asia.201801447

Temperature-sensitive luminescent materials have aroused great interest for practical applications in optical sensors. Layered rare-earth hydroxides (LRHs) possess rich interlayer chemistry and adjustable composition; thus, they are the promising candidates for designing functional materials, usually through an ion exchange process. Herein, the intercalation of neutral Tb^III complex rather than ion exchange was successfully performed in situ into the gallery of Y/Eu binary LRHs by using a hydrothermal process. Interestingly, the swollen LRHs are chameleon luminophores, exhibiting color emissions from green to pink that were tunable through variations in temperature ranging from 77 to 450 K. Because of the highly sensitive and temperature-dependent emissions, novel optical temperature sensors for 1D and 2D thermal imaging were fabricated by employing the chameleon luminophores, which displayed luminescence capable of reversibly undergoing repeated thermocycles. The present work opens up new fields in layered inorganic materials.

Full text of DOI:10.1002/asia.201801447

CHEMISTRY
AN ASIAN JOURNAL
www.chemasianj.org
Accepted Article
Title: Novel Luminescent Thermometry Developed by Y/Eu Binary
Layered Rare-Earth Hydroxide (LRH) via in Situ Intercalation with
Neutral Terbium (III) Complexes
Authors: Qi Zhu, Siyuan Li, Jianfeng Jin, Zhixin Xu, Xiaodong Li,
Xudong Sun, and Ji-Guang Li
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10.1002/asia.201801447
Chemistry - An Asian Journal
Novel Luminescent Thermometry Developed by Y/Eu Binary
Layered Rare-Earth Hydroxide (LRH) via in Situ Intercalation with
Neutral Terbium (Ⅲ) Complexes
Qi Zhu*, Siyuan Li, Jianfeng Jin, Zhixin Xu, Xiaodong Li, Xudong Sun, and Ji-Guang Li*
materials that are composed of positively charged hydroxide
layers of trivalent rare-earth ions, but are otherwise structurally
similar to hydrotalcite-type layered double hydroxides (LDHs).[1-5]
LRHs have recently been drawing keen research interest
because of their capacity to undergo intercalation and ion
exchange, which allow them to be used in a wide range of
applications, such as in rechargeable batteries, pollutant
trapping, heterogeneous catalysis, drug delivery, and
microelectronics.[6-10] The rich interlayer chemistry and the
adjustable composition of LRHs can be used to achieve
additional tunability to create numerous opportunities for
designing functional materials.[1a] Optical sensors for
temperature, in contrast to other thermometers, possess the
unique advantage of contactless measurement and large-scale
imaging.[11,12] Temperature-sensitive materials, especially
temperature-dependent luminescent materials, are candidates
for use in optical sensors.[13] Because luminescent lanthanide
complexes exhibit characteristic luminescence with narrow
emission bands and long emission lifetimes, they are suitable for
use in sensing devices.[14-18] Recently, a Eu (Ⅲ) complex was
Abstract:
Temperature-sensitive luminescent materials have aroused great
interest for practical applications in optical sensors. Layered rare-
earth hydroxides (LRHs) possess rich interlayer chemistry and
adjustable composition, thus they are the charming candidates for
designing functional materials, usually through an ion exchange
processing. Surprisingly, in this work, the intercalation of neutral Tb
(Ⅲ) complex rather than ion exchange was successfully performed
in situ into the gallery of Y/Eu binary LRHs by hydrothermal
processing. Interestingly, the swollen LRHs are chameleon
luminophore, exhibiting color emissions from green to pink that were
tunable through variations in temperature ranging from 77 to 450 K.
Because of the highly sensitive and temperature-dependent
emissions, novel optical temperature sensors for 1D and 2D thermal
imaging were fabricated by employing the chameleon luminophores,
which displayed luminescence capable of reversibly undergoing
repeated thermo-cycles. The present work opens up new fields in
layered inorganic materials.
Layered rare-earth hydroxides (LRHs) with a general formula of
RE2(OH)5(Am-)1/m·nH2O (RE: rare-earth ions; A: intercalated
anions) are a new group of important anion-type layered
successfully employed in
a polymer-based material for a
temperature-sensitive sensor.[14] However, it is difficult to
accurately measure temperature in extreme environments with
very low or very high temperatures due to the instability and
ineffectiveness of organic complexes in these environments.
Therefore, designing using hybrids of inorganic and organic
complexes are possible. Because coordination polymer
containing Tb (Ⅲ) ion and hfa (hexafluoro acetylacetonato)
ligands can exhibit effective energy back transfer from the
emitting level of the Tb (Ⅲ) ion to the excited triplet state of the
hfa ligand, the temperature-dependent green emission can be
observed.[14] Otherwise, the Tb (Ⅲ) to Eu (Ⅲ) energy transfer
may occur via exchange interaction and electric multipole
interaction, which depends on the distance between the Tb (Ⅲ)
donor and Eu (Ⅲ) acceptor ions.[19-21] If inserting the Tb (Ⅲ)
complexes into the gallery of Y/Eu binary LRHs, combining the
useful properties of energy back transfer in Tb (Ⅲ) complexes
and Tb (Ⅲ)→Eu (Ⅲ) energy transfer with the host-guest
chemistry, novel temperature-sensitive sensors based on the
[*]
Prof. Q. Zhu, S. Y. Li, Prof. J. F. Jin, Z. X. Xu, Prof. X. D. Li, Prof. X.
D. Sun
Key Laboratory for Anisotropy and Texture of Materials (Ministry of
Education)
Northeastern University
Shenyang, Liaoning 110819, China
E-mail: zhuq@smm.neu.edu.cn
Prof. Q. Zhu, S. Y. Li, Z. X. Xu, Prof. X. D. Li, Prof. X. D. Sun
Institute of Ceramics and Powder Metallurgy, School of Materials
Science and Engineering
Northeastern University
Shenyang, Liaoning 110819, China
Prof. X. D. Sun
School of Environmental and Chemical Engineering
Dalian University
Dalian, Liaoning 116622, China
Dr. J.-G. Li
Research Center for Functional Materials
National Institute for Materials Science
Namiki 1-1, Tsukuba, Ibaraki 305-0044, Japan
E-mail: LI.Jiguang@nims.go.jp
Supporting information for this article is given via a link at the end of
the document.((Please delete this text if not appropriate))
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10.1002/asia.201801447
Chemistry - An Asian Journal
new-formed layered compounds can be envisioned. However,
most of the previous studies focused on using LRHs as a
precursor for exfoliation into nanosheets or fabrication of
phosphor films.[1-5] The interlayer anions and molecules are
rarely used to modulate the functionalization. Recently, neutral
guest molecules, such as chloranil,[22] metolachlor,[23] and
fullerene (C60),[24] have been successfully inserted into the
galleries of Mg-Al double hydroxide anion-type layered
compounds and yielded hybrid materials, indicating the
possibility of insertion of neutral guest molecules into layered
compounds. However, previous studies largely focused on anion
exchanges by LRHs, while reports on intercalation with neutral
complexes have been rather limited.
Figure 1B shows the X-ray diffraction patterns of the LRH
and Tb(hfa)3(H2O)3-intercalated LRH (denoted as LRH-mTH)
obtained through various processes, which showed all samples
had typical ordered 2D lamellar stacked structures. Figure 1B(a)
displays a series of strong (00l) diffraction peaks indexed as
being in the LRH phase with a basal spacing of ~0.84 nm.[1-5]
The sizes and morphologies of the products were examined by
field emission scanning electron microscopy (FE-SEM) and
transmission electron microscopy (TEM) in Figure 2(a,e),
indicating the crystals had a plate-like morphology with a lateral
size of ~1 μm and thickness of ~70 nm. Figure 1B(b,c) show the
X-ray diffraction pattern of the LRH-0.5TH and LRH-TH samples
obtained through hydrothermal processing at 120 °C for 24 h in
the presence of 0.5-fold and 1-fold Tb(hfa)3(H2O)3. The (00l)
reflections, which were monitored as (002) and (004) reflections,
nearly kept at the same position. There is no obvious variation in
morphology for LRH-TH sample as shown in Figure 2 b,
indicating that intercalation of Tb(hfa)3(H2O)3 into the gallery did
not take place at the content of no more than 1-fold
Tb(hfa)3(H2O)3. However, the (00l) reflections shifted to the
lower-angle side and the basal spacing expanded to ~1.36 nm
for the LRH-1.5TH sample (Figure 1B(d)). Further increasing the
In the present work, the first intercalation of neutral Tb (Ⅲ)
complex (Tb(hfa)3(H2O)3) (Figure S1) was successfully
performed in situ into the gallery of Y/Eu binary LRHs by
hydrothermal processing (Figure 1A). Color tunable emissions
from green to pink were observed for the swollen LRHs at the
temperature ranging from 77 to 450 K. Becuase of the highly
sensitive and temperature-dependent emissions, novel optical
temperature sensors for thermal imaging have been constructed
using the swollen LRHs as buliding blocks.
Figure 1. (A) Schematic illustration for the intercalation of neutral Tb (III) complexes in situ into the gallery of LRH. (B) XRD
patterns and (C) FT-IR spectra of LRH (a), LRH-0.5TH (b), LRH-TH (c), LRH-1.5TH (d), LRH-2TH (e) and LRH-3TH (f).
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10.1002/asia.201801447
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Tb(hfa)3(H2O)3 from 1.5-fold to 3-fold resulted in no variation in
basal spacing (Figure 1B(e,f)). Figure 2(c,d,f) shows the typical
morphology of the LRH-mTH samples (m=2 and 3), where the
thickness of the LRH platelets significantly increased from ~70
nm to ~0.6 μm and even ~1.1 μm, with different gaps occurring
along the thickness due to the massive insertion of
Tb(hfa)3(H2O)3. Figure 1C shows the spectra obtained by Fourier
transform-infrared spectroscopy for the LRH and LRH-mTH. The
strong absorption peak at 1381 cm-1 is characteristic of an
uncoordinated nitrate anion and is comparable to peaks
observed for other layered hydroxides containing interlayer
nitrate groups (Figure 1B(a)).[25-26] After insertion of
Tb(hfa)3(H2O)3, vibration of the nitrate anion was still observed
for LRH-mYH, as shown in Figure 1C(b-f). The FT-IR spectra for
LRH and LRH-0.5YH samples are similar (Figure 1C(b)),
indicating no intercalation of Tb(hfa)3(H2O)3 into the gallery of
LRH. However, two bands located at ~1209 and ~1134 cm-1,
which were assigned to the stretching mode of C-F,[25-26] were
observed for LRH-TH sample, indicating the absorption of
Tb(hfa)3(H2O)3 on the sample surface. Stronger bands at ~1209
and ~1134 cm-1 were found for the LRH-mYH (m≥1.5) samples,
along with the intense band at ~1668 cm-1 assigned to the free
vibration of C=O.[25-26] But the double strong absorption peaks at
~1541 and ~1446 cm-1, due to the asymmetric and symmetric
stretching modes of C=O, indicated that some Tb(hfa)3(H2O)3 is
indirectly linked to the host layer via hydrogen bonding between
hydroxyls and carbonyls.[25-26] The above results showed that
insertion of Tb(hfa)3(H2O)3 into the gallery of LRH did not take
place until the Tb(hfa)3(H2O)3 increasing to 1.5-fold content,
indicating insertion of Tb(hfa)3(H2O)3 is a sudden process rather
Figure 2. FE-SEM and TEM micrographs showing morphologies of (a,e) LRH,
(b) LRH-TH, (c) LRH-2TH, and (d,f) LRH-3TH.
Becuase the swollen LRH-mTH (m=1.5-3) exibited simiar
luminescence behaviors (Figure S2), the LRH-3TH was taken
here as an example to investegate the luminescence property.
Figure S3 and Figure 3a show the photoluminescence excitation
(PLE)/photoluminescence (PL) spectra for swollen LRH-3TH.
The strong excitation bands with maxima at 243 nm indicated
that 243-nm excitation is the most efficient way for luminescence
(Figure S3). Upon UV excitation at 243 nm, the characteristic
emissions of both Tb (Ⅲ) and Eu (Ⅲ) simultaneously appeared
in the PL spectra (Figure 3a). Because LRH-3TH decomposes
at 210 oC (483 K, Figure S4), the heating T was set to a
maximum of 450 K (i.e., below 483 K) in this work. The green Tb
(Ⅲ) emission at 546 nm (5D4→7F5 transition of Tb (Ⅲ))
monotonically decreased as the temperature increased from 77
to 450 K. However, a higher temperature did not significantly
vary the intensity of Eu (Ⅲ) emissions at 617 nm (5D0→7F2
transition of Eu (Ⅲ)). As shown in Figure 3b, the
I(5D0→7F2)/I(5D4→7F5) intensity ratio (I546/I617) was analyzed as a
function of temperature. Clearly, the ratio decreased from ~2.82
at 77 K to ~1.26 at 450 K, indicating color-tunable emissions
from green to pink, as shown in Figures 3c and Figure S5.
Because the triplet state of hfa (22000 cm-1) is very close to the
emitting level of Tb (Ⅲ) ions (20500 cm-1), it resulted in effective
energy and energy-back transfer and, thus, high-performance
thermo-sensing.[16] Indeed, weakened luminenscence was found
for Tb(hfa)3(H2O)3 at a higher heating temperature (Figure S6).
than
a
gradual
one.
Chemical
analysis
for
identified
and
(Y0.996Eu0.004)2(OH)5.12(NO3)0.88·1.80H2O
LRH
(Y0.996Eu0.004)2(OH)5.14(NO3)0.86[Tb(C5F6O2H)3(H2O)3]1.34·2.65H2O
for LRH-3TH, indicating insertion of Tb(hfa)3(H2O)3 into the
gallery of LRH did not replace the nitrate anions.
In
previous
work,
the
coordination
polymer
[Tb0.99Eu0.01(hfa)3(dpbp)]n
displayed
temperature-sensing
luminescence, which were a result of effective energy and
energy-back transfer from Tb (Ⅲ) ions. The energy was
transferred to both the excited triplet state of the hfa ligands (i.e.,
energy-back transfer) and the Eu (Ⅲ) ions from the emitting
level of the Tb (Ⅲ) ions.[14] Shortened lifetime of Tb3+ emission
for LRH-3TH was found at a higher heating temperature (Figure
S7), which could be due to the energy transfer from Tb (Ⅲ) to
others. Becuase weakened intensity of Eu (Ⅲ) in LRH was
observed at a higher heating temperature (Figure S8), the
changeless intensity of Eu (Ⅲ) emissions for LRH-3TH in this
work indicated that the energy may both transfer from Tb (Ⅲ) to
the excited triplet state of the hfa ligands and the Eu (Ⅲ) with
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10.1002/asia.201801447
Chemistry - An Asian Journal
increasing temperature (Figure 3d). Furthermore, we
demonstrated the luminescence reversibly undergo repeated
thermo-cycles. The reversible changes of emission intensity
ratio of I(5D0→7F2)/I(5D4→7F5) are observed by the alternative
thermo-cycles in the range of 300 and 400 K (Figure S9). The
changes in the emission intensity ratio are stably repeated
between the I(5D0→7F2)/I(5D4→7F5) values of ~1.3 at 300 K and
~1.6 at 400 K.
This novel material with thermo-sensitive performance has
potential applications in optical temperature sensors. Sensing of
temperature via luminescence is almost exclusively based on
the use of luminescent molecular probes, nanoparticles or
aggregates.[12] The probes and sensors can be incorporated in
the sample to be studied, or deposited on its surface, usually in
the form of a two-dimensional film of a polymer host containing
the probes or particles.[12] In this work, swollen LRH-3TH
particles were selected for the temperature sensors, and LRH-
3TH/PVA rod (6 mm in diameter) and semi-transparent film
(0.10 mm in thickness) were successfully fabricated by solution
casting, with the preparation procedure schematically illustrated
in Figure 4A. Because of the high-performance thermo-sensing
of LRH-3TH/PVA, temperature distribution of the sample to be
studied can be easily obtained by analyzing the color through
the Matlab software (R2017b Version). The color contour was
made by Matlab software according to the RGB color contrast of
the treated sample. Firstly, the 1D sensor (LRH-3TH/PVA rod)
was partly put in liquid nitrogen with residual part in the air, and
the color distribution can be easily observed in Figure 4B in the
presence of
a 254-nm lamp excitation. The temperature
distribution along the one dimension direction was shown in
Figure 4B, and the results indicated that the temperature
distribution from liquid nitrogen region to air region did not strictly
follow the linear law. To verify the accuracy, the temperatures at
the 9-cm and 10.5-cm of the sensor were randomly tested, and
the results ~233 K and ~259 K are close to the modulated value
of ~235 K and 258 K. Because of the cooling effect resulted from
the volatile liquid nitrogen, the temperature around the sensor is
obvious lower than the room temperature (298 K). Due to the
excellent flexibility of the 2D sensor (LRH-3TH/PVA film), the film
sensor can be easily bent or shaped, which shows great
compatibility on curved or irregular surfaces and can accurately
exhibit the temperature distribution of the sample to be studied.
The 2D sensor was successfully applied on a designed cylinder
sample containing three temperature regions of 77 K, 277K, and
350 K. The color distribution of the cylinder sample was obtained
by excitation of a 254-nm lamp, and the visual temperature
distribution was shown in Figure 4C. The temperatures at 277-K
and 350-K regions were randomly tested, and the results ~281 K
and ~348 K are close to the modulated value of ~280 K and 345
K. Because interaction of the three temperature regions took
place, small deviation of practical temperatures were observed.
However, the close results indicated that the present sensors
have potential applications in optical sensors of temperature,
although further improvement is needed.
Figure 3. (a) PL spectra, (b) relative intensities of I546/I617 intensity ratio, (c)
emission colors (under 254 nm irradiation from a hand-held UV lamp) and (d)
energy transfer processes of the allachroic LRH-3TH, as a function of heating
temperature from 77 K to 450 K.
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Figure 4. (A) Preparation procedure of one-dimensional (1D) and two-dimensional (2D) optical temperature sensors and (B,C) their
applications in 1D and 2D thermal imaging. The photographs in A(c) and A(d) are the appearance of 1D and 2D sensors in day light and UV
irradiation, respectively. The blue asterisks in (B) and (C) are random test points obtained from the temperature sensors. The color for the
temperature distribution (right in C section) is fake color.
In summary, the first intercalation of neutral Tb (Ⅲ) complex
Acknowledgements
(Tb(hfa)3(H2O)3) was successfully performed in situ into the
gallery of Y/Eu binary LRHs by hydrothermal processing. The
expanded LRHs are chameleon luminophore that exhibited color
emissions from green to pink through increasing the temperature
from 77 to 450 K. 1D and 2D novel optical temperature sensors
for thermal imaging were prepared by dispersing the swollen
LRHs in PVA, which can undergo repeated thermo-cycles in
luminescence.
This work was supported in part by the Fundamental Research
Funds for the Central Universities (Grants N160204008 and
N172002001) and the National Natural Science Foundation of
China (Grant 51672039).
Keywords: layered rare-earth hydroxide, intercalation,
temperature-dependent
luminescence
emissions,
temperature
sensor,
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See the Supporting Information for details.
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Entry for the Table of Contents (Please choose one layout)
Layout 2:
COMMUNICATION
Qi Zhu*, Siyuan Li, Jianfeng Jin, Zhixin
Xu, Xiaodong Li, Xudong Sun, and Ji-
Guang Li*
Page No. – Page No.
Novel Luminescent Thermometry
Developed by Y/Eu Binary Layered
Rare-Earth Hydroxide (LRH) via in
Situ Intercalation with Neutral
Terbium (Ⅲ) Complexes
The first intercalation of neutral Tb (Ⅲ) complex is successfully performed in situ into the
gallery of LRH. Novel optical temperature sensors for 1D and 2D thermal imaging are
fabricated by employing the allachroic swollen LRHs, which opens up new fields in
layered inorganic materials.
This article is protected by copyright. All rights reserved.